Cyclopropylamine → HCID 178491237, 화합물

HRID 732106노트

반응식

HRID 732106 반응식
Cl.C(O[C:5](=[NH:14])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][CH:7]=1)C.[CH:15]1([NH2:18])[CH2:17][CH2:16]1>C(Cl)Cl>[CH:15]1([NH:18][C:5](=[NH:14])[C:6]2[CH:7]=[CH:8][C:9]([O:12][CH3:13])=[CH:10][CH:11]=2)[CH2:17][CH2:16]1

참가 물질

4

반응물 2

HCID 69828CyclopropylamineHCID 12270046Ethyl 4-methoxybenzimidate hydrochloride

생성물 1

HCID 178491237HCID 178491237, 화합물수율 82%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-methoxy-benzimidic acid ethyl ester hydrochloride (1.25 g, 5.8 mmol), DCM (5 ml) and cyclopropylamine (0.92 ml, 13.3 mmol) were mixed. After stirring at r.t for 3 h, the reaction mixture was concentrated in-vacuo. The residue was treated with cold aq. sodium hydroxide (1M) and extracted with EA. The combined organic phase was washed with water and brine, dried (Na2SO4), filtered and concentrated in-vacuo, to isolate the title compound (0.90 g, 82%). 1H-NMR: 7.64 (d, 2H), 6.90 (d, 2H), 5.3 (bs, 2H), 3.85 (s, 3H), 2.59 (m, 1H), 0.84 (m, 2H), 0.62 (m, 2H).

후처리

  1. concentrationthe reaction mixture was concentrated in-vacuo
  2. additionThe residue was treated with cold aq. sodium hydroxide (1M)
  3. extractionextracted with EA
  4. washThe combined organic phase was washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in-vacuo

출처 및 근거

ORD 기록
ord-7fad59dcafca4665b83f4718518a4c68
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585881B2

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